JPH0678164B2 - Manufacturing method of boehmite alumina - Google Patents
Manufacturing method of boehmite aluminaInfo
- Publication number
- JPH0678164B2 JPH0678164B2 JP1180639A JP18063989A JPH0678164B2 JP H0678164 B2 JPH0678164 B2 JP H0678164B2 JP 1180639 A JP1180639 A JP 1180639A JP 18063989 A JP18063989 A JP 18063989A JP H0678164 B2 JPH0678164 B2 JP H0678164B2
- Authority
- JP
- Japan
- Prior art keywords
- alumina
- hours
- stirring
- bar
- pressure
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Lifetime
Links
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- VXAUWWUXCIMFIM-UHFFFAOYSA-M aluminum;oxygen(2-);hydroxide Chemical compound [OH-].[O-2].[Al+3] VXAUWWUXCIMFIM-UHFFFAOYSA-M 0.000 title claims description 6
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 25
- 239000011148 porous material Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 13
- 239000000725 suspension Substances 0.000 claims description 11
- 230000032683 aging Effects 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- 230000002093 peripheral effect Effects 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 7
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 7
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 7
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims description 6
- 230000007062 hydrolysis Effects 0.000 claims description 6
- 238000006460 hydrolysis reaction Methods 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 5
- 238000010586 diagram Methods 0.000 description 5
- 239000002002 slurry Substances 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000009826 distribution Methods 0.000 description 4
- 238000001694 spray drying Methods 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 239000012535 impurity Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000002360 preparation method Methods 0.000 description 2
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 description 1
- 229910000013 Ammonium bicarbonate Inorganic materials 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 description 1
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 description 1
- 235000012538 ammonium bicarbonate Nutrition 0.000 description 1
- 239000001099 ammonium carbonate Substances 0.000 description 1
- 238000001354 calcination Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- FAHBNUUHRFUEAI-UHFFFAOYSA-M hydroxidooxidoaluminium Chemical group O[Al]=O FAHBNUUHRFUEAI-UHFFFAOYSA-M 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 150000004682 monohydrates Chemical class 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 229910001388 sodium aluminate Inorganic materials 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/44—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water
- C01F7/447—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes
- C01F7/448—Dehydration of aluminium oxide or hydroxide, i.e. all conversions of one form into another involving a loss of water by wet processes using superatmospheric pressure, e.g. hydrothermal conversion of gibbsite into boehmite
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/14—Pore volume
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/16—Pore diameter
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/22—Rheological behaviour as dispersion, e.g. viscosity, sedimentation stability
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geology (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Catalysts (AREA)
- Silicates, Zeolites, And Molecular Sieves (AREA)
Description
【発明の詳細な説明】 〔産業上の利用分野〕 本発明は,3〜100nmの範囲内に気孔半径が調節可能でAl2
O3純度が少くとも99.95％のベーマイトアルミナの製造
方法に関する。DETAILED DESCRIPTION OF THE INVENTION [Industrial field of application] The present invention has an adjustable pore radius of Al 2 within a range of 3 to 100 nm.
The present invention relates to a method for producing boehmite alumina having an O 3 purity of at least 99.95%.
例えばドイツ特許第1258854号によるアルミニウムアル
コラートの中性加水分解によれば，ベーマイト構造のア
ルミナ又はα−アルミナ酸化物一水化物が取得される。
この生成物は，最大気孔半径が２〜4nmであり，顔料，
充填剤，研摩剤又は触媒担体として用いられる。しか
し，触媒の担体物質の場合，又は，気体成分の分離用に
は，気孔の容積又は半径が特定の範囲に含まれる前記ア
ルミナが取得されることが特に望ましい。できる限り狭
い気孔半径の分布を保ちながら，アルミナの気孔の容積
並びにその半径を増大させることが特に望ましい。For example, neutral hydrolysis of aluminum alcoholates according to German Patent No. 1258854 yields alumina or α-alumina oxide monohydrate with a boehmite structure.
This product has a maximum pore radius of 2 to 4 nm,
Used as filler, abrasive or catalyst carrier. However, in the case of catalyst support materials or for the separation of gaseous components, it is particularly desirable to obtain the alumina whose pore volume or radius lies within a certain range. It is especially desirable to increase the pore volume and the radius of the alumina while maintaining the pore radius distribution as narrow as possible.
最大の気孔半径を得るには，例えばドイツ特許第255680
4号に従って炭酸水素アンモニウムを添加したり，ドイ
ツ特許第2314350号に従ってC1〜C4アルコールで処理し
たり，ドイツ特許第2932648号に従って沈殿の間にpH値
を反復変化させたりして，気孔の半径又は容積を増大さ
せることができる。これらの方法によれば不純物が導入
されることはさておき，これらの方法は，計画されたよ
うに明確に限定された気孔の半径の分布を得ることを可
能としない。沈殿させたアルミナのエージングによっ
て，結晶を成長させ，それによって気孔の半径を増大さ
せることは，英国特許第1169096号及び第1226012号によ
って公知となっている。しかし硝酸と共にアルミン酸ナ
トリウムから沈殿させるこれらのアルミナの場合にも，
非常に広い気孔の最大値が，約７日間に亘る長い予備的
なエージングと次いで210℃〜220℃での15時間の仮焼の
後に始めて得られるにすぎない。To obtain the maximum pore radius, for example, German Patent No. 255680
The addition of ammonium hydrogen carbonate according to DE 4 , the treatment with C 1 -C 4 alcohols according to DE 2314350 and the repeated change of the pH value during precipitation according to DE 2932648 lead to the formation of pores The radius or volume can be increased. Apart from the introduction of impurities by these methods, these methods do not make it possible to obtain a well-defined distribution of pore radii as planned. It is known from British Patent Nos. 1169096 and 1226012 to grow crystals and thereby increase the pore radius by aging the precipitated alumina. However, in the case of these aluminas which are precipitated from sodium aluminate with nitric acid,
Very wide pore maximums are only obtained after long preliminary aging for about 7 days and then 15 hours of calcination at 210 ° -220 ° C.
本発明の課題は，計画された調節可能な気孔半径分布を
示すベーマイトアルミナ即ちα−アルミニウムオキサイ
ド一水化物を高純度レベルにおいて産業的な規模で好ま
しくは連続的に製造することにある。The object of the present invention is to produce boehmite alumina or α-aluminium oxide monohydrate with a planned and adjustable pore radius distribution, preferably at high purity levels on an industrial scale, preferably continuously.
本発明によれば，この課題は，請求項１に示した製造方
法によって解決される。即ち，本発明は,3〜100nmの範
囲に気孔半径が調節可能でAl2O3純度が少くとも99.95％
のベーマイトアルミナの製造方法において， 中性アルミニウムアルコラートの加水分解からのアルミ
ナ懸濁液をオートクレーブ中において ａ）100〜235℃の温度に対応して１〜30バールの水蒸気
圧力において ｂ）0.5〜20時間に亘って ｃ）1.0〜6.0m/秒の周速で撹拌しつつ、 エージングを行なうことを特徴とする。According to the invention, this problem is solved by the manufacturing method according to claim 1. That is, according to the present invention, the pore radius can be adjusted within the range of 3 to 100 nm, and the Al 2 O 3 purity is at least 99.95%.
In the process for the preparation of boehmite alumina according to 1., the alumina suspension from the hydrolysis of neutral aluminum alcoholate is a) in an autoclave a) at a steam pressure of 1-30 bar corresponding to a temperature of 100-235 ° C b) 0.5-20 Aging is performed while stirring at a peripheral speed of 1.0 to 6.0 m / sec over time c).
本発明の好ましい実施態様について，請求項２以下に特
許請求する。A preferred embodiment of the present invention is claimed in claims 2 and below.
驚くべきことに，中性アルミニウムアルコラートの加水
分解から得られるアルミナ懸濁液を後処理するための，
所定の工程条件の下において,100°〜235℃の温度に対
応する水蒸気圧力１〜30バール（1.02〜30.6kgf/cm2）
において，特に150〜215℃の温度に対応する水蒸気圧５
〜20バール（5.1〜20.4kgf/cm2）において,0.5〜20時
間，好ましくは１〜４時間エージングが行ない，好まし
くは５〜15重量％のAl2O3を含有する懸濁液を処理する
と，所望の純度と特定の気孔半径とを備えたベーマイト
アルミナが取得されることが見出された。また，特に驚
くべきことに,1.0〜6.0m/秒，好ましくは1.15〜5.2m/秒
の周速によって表わされる撹拌度を用いることによっ
て，所望の気孔半径の最大値が得られる。Surprisingly, for the aftertreatment of the alumina suspension obtained from the hydrolysis of neutral aluminum alcoholates,
Steam pressure 1 to 30 bar (1.02 to 30.6 kgf / cm 2 ) corresponding to a temperature of 100 ° to 235 ° C under specified process conditions
In particular, water vapor pressure 5 corresponding to the temperature of 150-215 ℃
Aging at 0.5 to 20 bar (5.1 to 20.4 kgf / cm 2 ) for 0.5 to 20 hours, preferably 1 to 4 hours, preferably treating a suspension containing 5 to 15 wt% Al 2 O 3 It has been found that boehmite alumina with desired purity and specific pore radius is obtained. Also, surprisingly, by using a stirring degree represented by a peripheral speed of 1.0 to 6.0 m / sec, preferably 1.15 to 5.2 m / sec, the desired maximum pore radius can be obtained.
２〜10段，好ましくは４〜10段のカスケード反応器によ
って撹拌を行なうことが好ましく，より適切には，無段
に調節可能な撹拌装置を備えた反応器を使用する。It is preferable to carry out the stirring by a cascade reactor having 2 to 10 stages, preferably 4 to 10 stages, and more suitably, a reactor equipped with a continuously adjustable stirring device is used.
次に本発明を実施例に基づいて一層詳細に説明する。Next, the present invention will be described in more detail based on examples.
実施例１ 次のようにして作製した，中性のアルミニウムアルコラ
ートの加水分解から得たアルミナ懸濁液（サスペンショ
ン）ないしスラリーを，出発物質として使用した。例え
ばチーグラー／アルフォール法による合成法の際に中間
体として得られるようなアルミニウムアルコラート混合
物を撹拌装置つきの容器中において，不純物イオンを完
全脱イオン装置によって完全に除去した水で90℃で加水
分解した。この際に２つの互に混和しない相即ち上部の
アルコール相と下部のアルミナ／水相とが形成された。
アルミナ／水相は，Al2O3含量が10〜11％の水酸化アル
ミニウムを含有していた。アルコラート混合物の代りに
純アルミニウムアルコラートを使用してもよい。この加
水分解は一般に30〜110℃，好ましくは60〜100℃の範囲
で行なうことができる。Example 1 An alumina suspension (suspension) or slurry obtained by hydrolysis of a neutral aluminum alcoholate prepared as follows was used as a starting material. For example, an aluminum alcoholate mixture obtained as an intermediate in the synthesis by the Ziegler / Alfort method was hydrolyzed at 90 ° C in a vessel equipped with a stirrer with water in which impurity ions were completely removed by a complete deionizer. . Two immiscible phases were formed during this, an upper alcohol phase and a lower alumina / water phase.
The alumina / water phase contained aluminum hydroxide with an Al 2 O 3 content of 10-11%. Pure aluminum alcoholate may be used in place of the alcoholate mixture. This hydrolysis can be carried out generally in the range of 30 to 110 ° C, preferably 60 to 100 ° C.
バッチ式の操作の場合には，Al2O3を10〜11重量％含有
するこのアルミナ懸濁液50kgを反応器に装入し，反応器
を125℃に対応する５バール（5.1kgf/cm2）とした。反
応条件を設定した後，撹拌装置の速度200rpmに対応する
周速2.30m/秒で普通の撹拌装置を使用して,0.5時間のエ
ージングを行なった。550℃×３時間の試料の調製後に
水銀気孔径測定法によって気孔半径分布を通常のように
累積的に測定した。評価の目的のために次式を使用し
た。In the case of batch operation, 50 kg of this alumina suspension containing 10 to 11% by weight of Al 2 O 3 was charged into the reactor and the reactor was operated at 5 bar (5.1 kgf / cm 2 corresponding to 125 ° C). 2 ) After setting the reaction conditions, aging was performed for 0.5 hours using an ordinary stirring device at a peripheral speed of 2.30 m / sec corresponding to a stirring device speed of 200 rpm. After preparation of the sample at 550 ° C. for 3 hours, the pore radius distribution was cumulatively measured by a mercury pore size measuring method as usual. The following equation was used for evaluation purposes.
Ｄ＝−｛（1/P）・4cosθ｝ 式においてＤは，気孔の直径,Pは圧力，θは接触角であ
る。D =-{(1 / P) · 4cosθ} In the equation, D is the diameter of the pore, P is the pressure, and θ is the contact angle.
スラリーの噴射乾燥後に，下記表１に示すデータを得
た。The data shown in Table 1 below were obtained after spray drying the slurry.
実施例２ 滞留時間を２倍の１時間とし，反応器の圧力を15バール
（15.3kgf/cm2）とし，温度を198℃としたことを除いて
は，実施例１と同一の手順に従った。 Example 2 The same procedure as in Example 1 was followed except that the residence time was doubled for 1 hour, the reactor pressure was 15 bar (15.3 kgf / cm 2 ) and the temperature was 198 ° C. It was
撹拌速度即ち撹拌装置の回転速度を200rpmとし，撹拌装
置の周速を2.30m/秒とした。スラリーの噴射乾燥後に下
記表２に示す分析データを得た。The stirring speed, that is, the rotation speed of the stirring device was 200 rpm, and the peripheral speed of the stirring device was 2.30 m / sec. The analytical data shown in Table 2 below were obtained after spray drying the slurry.
実施例３ 反応装置の条件を設定した後，滞留時間を３時間とした
ことを除いて，実施例1,2と同様に反応を行なわせた。
反応装置の圧力は23バール（23.5kgf/cm2），温度は220
℃であった。 Example 3 After setting the conditions of the reactor, the reaction was carried out in the same manner as in Examples 1 and 2 except that the residence time was 3 hours.
The reactor pressure is 23 bar (23.5 kgf / cm 2 ) and the temperature is 220.
It was ℃.
下記表３に示す測定結果を得た。The measurement results shown in Table 3 below were obtained.
滞留時間及び圧力の関数としての，実施例１〜３によっ
て得た気孔半径を，第1,2図に示す。これらの図からわ
かるように，連続撹拌をもってエージングする際に，ア
ルミナの気孔径の最大値を滞留時間及び圧力の関数とし
て正確に設定することができる。 The pore radii obtained according to Examples 1 to 3 as a function of residence time and pressure are shown in FIGS. As can be seen from these figures, the maximum value of the pore size of alumina can be accurately set as a function of the residence time and the pressure when aging with continuous stirring.
実施例４ Al2O3の濃度が約10重量％の実施例１によるアルミナ懸
濁液を，第３図による反応器に連続的に装入し，撹拌し
た。第３図に示す反応器（オートクレーブ）は，カスケ
ードに配列された５つの撹拌段を備えている。上方から
配管２及びポンプ４を経て反応器６にアルミナスラリー
を装入し，それと同時に高圧蒸気を配管８により供給し
た。撹拌装置は電動機10によって駆動され，この実施例
では，トレーないし板を介在させた５個のカスケード配
列で重ね合せ配列の撹拌装置12a〜12eを備えており，こ
れらのトレーないし板によって１つのカスケード室から
その下方の室への制御された通過を可能にする。レベル
調整器14といくつかの温度センサー16,16′とによっ
て，一様な反応連鎖を確実に保持できる。スラリーの進
入と水蒸気の供給とは，排出弁18により制御される排出
量の関数として制御する。Example 4 The alumina suspension of Example 1 having a concentration of Al 2 O 3 of about 10% by weight was continuously charged into the reactor of FIG. 3 and stirred. The reactor (autoclave) shown in FIG. 3 is equipped with five stirring stages arranged in a cascade. Alumina slurry was charged into the reactor 6 from above through the pipe 2 and the pump 4, and at the same time, high-pressure steam was supplied through the pipe 8. The stirrer is driven by an electric motor 10, and in this embodiment, it is equipped with stirrers 12a to 12e in a stack of five cascades with trays or plates interposed, and these trays or plates form one cascade. Allows controlled passage from the chamber to the chamber below it. A level regulator 14 and several temperature sensors 16, 16 'ensure that a uniform reaction chain is maintained. Slurry ingress and water vapor delivery are controlled as a function of emissions controlled by the exhaust valve 18.
この例においての滞留時間は,1,2及び３時間であった。
反応圧力は,212℃において20バール（20.4kgf/cm2）で
あった。撹拌装置12の速度，従って，撹拌装置の周速は
対応して変化させ，噴霧乾燥を行なった後，表４に示す
特性のアルミナが得られた。The residence time in this example was 1, 2 and 3 hours.
The reaction pressure was 20 bar (20.4 kgf / cm 2 ) at 212 ° C. The speed of the stirrer 12, and thus the peripheral speed of the stirrer, was correspondingly changed, and after spray drying, alumina having the characteristics shown in Table 4 was obtained.
実施例５ 圧力を15バール（15.3kgf/cm2），滞留時間を２時間と
した以外は，実施例４と同様に操作を行なった。表５に
対応した値を示す。第4,5図の線図は実施例4,5に対応し
ている。Example 5 The same operation as in Example 4 was carried out except that the pressure was 15 bar (15.3 kgf / cm 2 ) and the residence time was 2 hours. Table 5 shows the corresponding values. The diagrams in FIGS. 4 and 5 correspond to Examples 4 and 5.
第１図は，エージングの間の圧力及び滞留時間の関数と
してのアルミナの気孔半径の最大値を示す線図，第２図
は，エージングの間の水蒸気圧力及び滞留時間の関数と
してのアルミナの気孔半径の最大値を示す線図，第３図
は，本発明の製造方法に使用する反応器を示す概略配列
図，第４図は，水蒸気圧力を一定とした場合の周速及び
滞留時間の関数としてのアルミナの気孔半径の最大値を
示す線図，第５図は，滞留時間を一定とした場合の周速
及び水蒸気圧力の関数としてのアルミナの気孔半径の最
大値を示す線図である。Figure 1 shows the maximum pore radius of alumina as a function of pressure and residence time during aging, and Figure 2 shows the pores of alumina as a function of water vapor pressure and residence time during aging. A diagram showing the maximum value of the radius, FIG. 3 is a schematic arrangement diagram showing the reactor used in the production method of the present invention, and FIG. 4 is a function of the peripheral velocity and the residence time when the steam pressure is constant. 5 is a diagram showing the maximum value of the pore radius of alumina, and FIG. 5 is a diagram showing the maximum value of the pore radius of alumina as a function of the peripheral speed and the steam pressure when the residence time is constant.
───────────────────────────────────────────────────── フロントページの続き (72)発明者 アンスガー・ライヘナウァー 西ドイツ 2222 マルネ、フェルトシュト ラーセ 55 (56)参考文献 特開 昭53−119800（ＪＰ，Ａ) 特公 昭57−44605（ＪＰ，Ｂ２) ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Ansgar Reichenauer West Germany 2222 Marne, Feldstraße 55 (56) References JP-A-53-119800 (JP, A) JP-B 57-44605 (JP, B2)
Claims (4)
l2O3純度が少くとも99.95％のベーマイトアルミナの製
造方法において， 中性アルミニウムアルコラートの加水分解からのアルミ
ナ懸濁液をオートクレーブ中において ａ）100〜235℃の温度に対応して１〜30バールの水蒸気
圧力において ｂ）0.5〜20時間に亘って ｃ）1.0〜6.0m/秒の周速で撹拌しつつ エージングを行なうことを特徴とする製造方法。1. The pore radius can be adjusted within the range of 3 to 100 nm.
In l 2 O 3 production method of purity at least 99.95% of boehmite alumina, with the alumina suspension from the hydrolysis of neutral aluminum alcoholate corresponding to the temperature of a) one hundred to two hundred thirty-five ° C. in an autoclave 30 A manufacturing method characterized by performing baging for 0.5 to 20 hours at a steam pressure of bar, and c) aging while stirring at a peripheral speed of 1.0 to 6.0 m / sec.
を使用することを特徴とする請求項１記載の製造方法。2. The production method according to claim 1, wherein an alumina suspension containing 5 to 15% by weight of Al 2 O 3 is used.
請求項１又は２記載の製造方法。3. The process according to claim 1, wherein a) the alumina suspension is aged under a water vapor pressure of 5 to 30 bar and b) with stirring for 1 to 4 hours.
応器においてアルミナ懸濁液を連続的にエージングする
ことを特徴とする請求項１〜３のいずれか１項記載の製
造方法。4. The production method according to claim 1, wherein the alumina suspension is continuously aged in a cascade reactor equipped with a stirrer having 2 to 10 stages.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| DE3823895.0 | 1988-07-14 | ||
| DE3823895A DE3823895C1 (en) | 1988-07-14 | 1988-07-14 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| JPH0264010A JPH0264010A (en) | 1990-03-05 |
| JPH0678164B2 true JPH0678164B2 (en) | 1994-10-05 |
Family
ID=6358672
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP1180639A Expired - Lifetime JPH0678164B2 (en) | 1988-07-14 | 1989-07-14 | Manufacturing method of boehmite alumina |
Country Status (8)
| Country | Link |
|---|---|
| US (1) | US5055019A (en) |
| JP (1) | JPH0678164B2 (en) |
| BE (1) | BE1001847A3 (en) |
| DE (1) | DE3823895C1 (en) |
| FR (1) | FR2634194B1 (en) |
| GB (1) | GB2220651B (en) |
| IT (1) | IT1230055B (en) |
| NL (1) | NL194792C (en) |
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- 1988-07-14 DE DE3823895A patent/DE3823895C1/de not_active Expired
-
1989
- 1989-04-13 NL NL8900924A patent/NL194792C/en not_active IP Right Cessation
- 1989-04-13 IT IT8920124A patent/IT1230055B/en active
- 1989-04-24 BE BE8900454A patent/BE1001847A3/en not_active IP Right Cessation
- 1989-05-16 GB GB8911178A patent/GB2220651B/en not_active Expired - Lifetime
- 1989-05-22 FR FR8906632A patent/FR2634194B1/en not_active Expired - Lifetime
- 1989-06-02 US US07/360,311 patent/US5055019A/en not_active Expired - Lifetime
- 1989-07-14 JP JP1180639A patent/JPH0678164B2/en not_active Expired - Lifetime
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|---|---|---|---|---|
| JP5744605B2 (en) | 2011-04-07 | 2015-07-08 | キヤノン株式会社 | Information processing apparatus and information processing method |
Also Published As
| Publication number | Publication date |
|---|---|
| GB2220651B (en) | 1992-01-22 |
| FR2634194A1 (en) | 1990-01-19 |
| GB8911178D0 (en) | 1989-07-05 |
| IT8920124A0 (en) | 1989-04-13 |
| JPH0264010A (en) | 1990-03-05 |
| BE1001847A3 (en) | 1990-03-20 |
| GB2220651A (en) | 1990-01-17 |
| NL8900924A (en) | 1990-02-01 |
| NL194792B (en) | 2002-11-01 |
| IT1230055B (en) | 1991-09-27 |
| NL194792C (en) | 2003-03-04 |
| DE3823895C1 (en) | 1989-12-21 |
| FR2634194B1 (en) | 1993-03-19 |
| US5055019A (en) | 1991-10-08 |
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